Mesoporous nickel intercalated aluminosilicate nanohybrid has been synthesized through a recombination reaction between the colloidal suspension of exfoliated montmorillonite nanosheets and aqueous nickel acetate solution. According to powder X-ray diffraction and field emission-scanning electron microscopic analyses, the intercalation of nickel species expands significantly the basal spacing of the host montmorillonite clay and the crystallites of the intercalation compound are assembled to form a house-of-card structure. $N_2$ adsorption-desorption isotherm measurements with BJH pore analyses clearly demonstrated that the porosity of the intercalate originates mainly from mesopores (diameter $sim50;AA$) formed by the house-of-card type stacking of clay crystallites. From FT-IR and X-ray absorption spectroscopic analyses, it becomes certain that intercalated nickel ion is stabilized in an isolated $NiO_6$ octahedral unit. The present mesoporous intercalation compound is expected to be applicable as efficient catalysts or absorbents.